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Atomic layer deposition processes for the formation of ruthenium films, and ruthenium precursors useful in such processes

a technology of atomic layer deposition and ruthenium, which is applied in the direction of chemically reactive gas growth, crystal growth process, polycrystalline material growth, etc., can solve the problems of contaminated ru metal film fragments degraded, uncompatibility of oxygen with some barrier layer used in electronic device manufacturing, and inability to meet the requirements of oxygen-based barrier layer,

Inactive Publication Date: 2009-12-15
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention provides a process for depositing an oxide-free ruthenium-containing film on a substrate surface. This involves exposing the surface to a surface-activating agent to form a deposit of a surface-activating complex, then exposing this complex to a ruthenium precursor and a reducing agent to form the ruthenium complex. The resulting film is free of oxides and can be used in various applications. The invention also includes ruthenium complexes that can be used as ruthenium precursors in the deposition process.

Problems solved by technology

Often, these processes produce films contaminated with fragments from the metal ligands degraded during the thermal deposition.
The growth temperature of the metal thin film is approximately 200-500° C., preferably 300-360° C. One disadvantage of the process is that oxygen is not compatible with some barrier layers that are used in the manufacture of electronic devices.
Another disadvantage is that the deposited Ru metal film may contain unacceptably high levels of contaminants derived from the oxidation of the precursor ligands.

Method used

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  • Atomic layer deposition processes for the formation of ruthenium films, and ruthenium precursors useful in such processes
  • Atomic layer deposition processes for the formation of ruthenium films, and ruthenium precursors useful in such processes
  • Atomic layer deposition processes for the formation of ruthenium films, and ruthenium precursors useful in such processes

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0064]This Example demonstrates the preparation of bis(acetonitrile)bis(2,2,6,6-tetramethylheptanedionato)ruthenium(III) tetrafluoroethanesulfonate, ([RuL2(CH3CN)2]TFES).

[0065]In a Vacuum Atmospheres dry box under a nitrogen atmosphere, tris(2,2,6,6-tetramethyl-3,5-heptanedinato)ruthenium(III) (2.00 g) was dissolved in 50 mL acetonitrile. Tetrafluoroethanesulfonic acid (0.687 g) was dissolved in 2-3 mL acetonitrile and added in portions over 5-10 min to a stirred solution of the ruthenium complex in acetonitrile. A deep purple color developed immediately. The solution was stirred for one hour at room temperature. The solvent volume was reduced to 5-10 mL under vacuum. The dark blue solution was removed from the dry box, dissolved in 100 mL dichloromethane, and extracted three times with 100 mL ion chromatography grade water. The organic layer was then dried over anhydrous magnesium sulfate and filtered. The solvents were removed on a rotary evaporator. The dark solid was returned to...

example 2

[0066]This Example demonstrates the preparation of (N-acetimidoylacetamidinato)bis(2,2,6,6-tetramethylheptanedionato)ruthenium(III), [RuL2(C4H8N3)].

[0067]In the dry box, 1.50 g of [Ru(2,2,6,6-tetramethylheptanedionato)2(CH3CN)2]TFES prepared as in Example 1 was dissolved in approximately 25 mL acetonitrile. To this solution was added an ammonia solution in methanol (4 mL of a 2.0 M solution). The mixture was stirred for four days at room temperature. During this time, the solution color changed from bluish purple to reddish purple. Solvent was removed under vacuum to yield a dry, reddish-purple solid, [Ru(C11H19O2)2(C4H9N3)]TFES. Infrared spectrum in a Nujol mull shows stretches at 3437, 3264, and 3211 cm−1 (N—H stretch), 1654 cm−1 (C═N stretch), 1583, 1530, and 1499 cm−1 (C═O stretch) and 1248 cm−1 (S—O stretch). To 1.00 g of this product in 25 mL of acetonitrile was added sodium methoxide (0.076 g) as a powder. The reaction mixture was stirred at room temperature for 0.5 hr. The s...

example 3

[0068]This Example demonstrates the preparation of N,N′-diethylpentanediketimato)bis(2,2,6,6-tetramethylheptanedionato)ruthenium(III), [RuL2(C9H17N2)].

[0069]All manipulations were performed in a Vacuum Atmosphere dry box under nitrogen. [Ru(2,2,6,6-tetramethylheptanedionato)2(CH3CN)2]TFES, (0.140 g) prepared as described in Example 1 was dissolved in approximately 10 mL acetonitrile in a 20-mL screw-top vial. A Teflon®-coated stir bar was added. 0.0295 g Li (N,N′-diethylpentanediketiminate), prepared by the reaction of the free ligand and t-butyl lithium in ether (US 2005 / 0227007), was added all at once as a dry powder. Within minutes, the solution color changed from a bluish purple to red. The mixture was stirred at room temperature for 0.5 hr. The solvent was removed under vacuum. The residues were extracted with hexanes. Filtration yielded a red solution. Solvent was removed under vacuum to yield a red oil.

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Abstract

This invention is directed to processes for the formation of ruthenium-containing films on surfaces in atomic layer deposition (ALD) processes. The ALD process includes depositing a surface-activating group on the surface; exposing the deposit of the surface-activating complex to a ruthenium precursor to form a deposited ruthenium complex on the surface; and reacting the deposited ruthenium complex with a reducing agent to form a ruthenium-containing film on the surface. This invention is also directed to ruthenium complexes, RuL2L*, that can be used as ruthenium precursors in these processes.

Description

FIELD OF THE INVENTION[0001]This invention relates to processes for the formation of ruthenium-containing films on surfaces in atomic layer deposition (ALD) processes using surface-activating agents, and to ruthenium complexes that can be used as ruthenium precursors in these processes.BACKGROUND[0002]Atomic layer deposition (ALD), also known as atomic layer epitaxy, is a process for depositing highly uniform and conformal thin layers of a metal on a surface. The surface is exposed to vapors of the metal precursor and a reducing agent. Such films have a wide variety of applications in semiconductor microelectronics and optical films. The conventional ALD process, which uses a two-step procedure, is described by M. Ritala and M. Leskela in “Atomic Layer Deposition” in Handbook of Thin Film Materials, H. S. Nalwa, Editor, Academic Press, San Diego, 2001, Volume 1, Chapter 2.[0003]In a typical two-step ALD process, there is a self-limiting adsorption of the metal complex to the surface...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): C30B25/00C23C16/18
CPCC23C16/02C23C16/18H01L21/76873C23C16/45534H01L21/28562C23C16/45525C23C16/455
Inventor THOMPSON, JEFFERY SCOTT
Owner EI DU PONT DE NEMOURS & CO
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